# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Morris, R.'
'Prokopchuk, Demyan'
'Lough, Alan'
_publ_contact_author_name 'Morris, R.'
_publ_contact_author_email rmorris@chem.utoronto.ca
_publ_section_title
;
From Amine to Alkylamine to Azaallyl: Unusual
Transformation of Di-(2-pyridylmethyl)amine on
Ruthenium
;
# Attachment '- 1.cif'
data_k10161
_database_code_depnum_ccdc_archive 'CCDC 821591'
#TrackingRef '- 1.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H44 N3 P2 Ru, Cl'
_chemical_formula_sum 'C48 H44 Cl N3 P2 Ru'
_chemical_formula_weight 861.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.0768(3)
_cell_length_b 33.8502(12)
_cell_length_c 12.4059(2)
_cell_angle_alpha 90.00
_cell_angle_beta 91.6730(16)
_cell_angle_gamma 90.00
_cell_volume 4649.6(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 17710
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.230
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1776
_exptl_absorpt_coefficient_mu 0.497
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.731
_exptl_absorpt_correction_T_max 0.930
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 29446
_diffrn_reflns_av_R_equivalents 0.115
_diffrn_reflns_av_sigmaI/netI 0.152
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -40
_diffrn_reflns_limit_k_max 40
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.00
_reflns_number_total 8097
_reflns_number_gt 3903
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1203P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8097
_refine_ls_number_parameters 471
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1630
_refine_ls_R_factor_gt 0.0730
_refine_ls_wR_factor_ref 0.2182
_refine_ls_wR_factor_gt 0.1776
_refine_ls_goodness_of_fit_ref 0.930
_refine_ls_restrained_S_all 0.930
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.24159(5) 0.115158(18) 0.44329(4) 0.0330(2) Uani 1 1 d . A .
H1RU H 0.351(6) 0.152(2) 0.461(5) 0.07(2) Uiso 1 1 d . . .
Cl1 Cl -0.12500(17) 0.04511(6) 0.33215(17) 0.0545(6) Uani 1 1 d . . .
P1 P 0.23101(16) 0.12750(6) 0.26151(14) 0.0327(5) Uani 1 1 d . . .
P2 P 0.13191(16) 0.16914(6) 0.49148(14) 0.0350(5) Uani 1 1 d . . .
N1 N 0.3625(5) 0.06781(19) 0.4137(4) 0.0346(15) Uani 1 1 d . . .
N2 N 0.1235(4) 0.06206(17) 0.4586(4) 0.0325(14) Uani 1 1 d . . .
H2B H 0.0519 0.0665 0.4195 0.039 Uiso 1 1 calc R A .
N3 N 0.2693(5) 0.0986(2) 0.6062(5) 0.0429(16) Uani 1 1 d . . .
C1 C 0.4815(6) 0.0732(3) 0.4004(5) 0.047(2) Uani 1 1 d . A .
H1A H 0.5146 0.0989 0.4093 0.056 Uiso 1 1 calc R . .
C2 C 0.5588(7) 0.0416(3) 0.3736(6) 0.057(2) Uani 1 1 d . . .
H2A H 0.6424 0.0459 0.3634 0.069 Uiso 1 1 calc R A .
C3 C 0.5098(8) 0.0052(3) 0.3628(6) 0.059(3) Uani 1 1 d . A .
H3A H 0.5598 -0.0166 0.3453 0.071 Uiso 1 1 calc R . .
C4 C 0.3889(7) -0.0008(3) 0.3771(6) 0.051(2) Uani 1 1 d . . .
H4A H 0.3545 -0.0264 0.3697 0.061 Uiso 1 1 calc R A .
C5 C 0.3185(6) 0.0312(2) 0.4022(5) 0.0358(18) Uani 1 1 d . A .
C6 C 0.1838(7) 0.0265(2) 0.4136(6) 0.048(2) Uani 1 1 d . A .
H6A H 0.1467 0.0206 0.3418 0.057 Uiso 1 1 calc R . .
H6B H 0.1687 0.0037 0.4611 0.057 Uiso 1 1 calc R . .
C7 C 0.0952(6) 0.0579(2) 0.5745(5) 0.048(2) Uani 1 1 d . A .
H7A H 0.0239 0.0743 0.5903 0.057 Uiso 1 1 calc R . .
H7B H 0.0746 0.0300 0.5897 0.057 Uiso 1 1 calc R . .
C8 C 0.1980(7) 0.0701(2) 0.6456(5) 0.0398(19) Uani 1 1 d . A .
C9 C 0.2154(8) 0.0542(3) 0.7478(6) 0.056(2) Uani 1 1 d . . .
H9A H 0.1652 0.0335 0.7723 0.067 Uiso 1 1 calc R A .
C10 C 0.3065(9) 0.0690(3) 0.8127(7) 0.065(3) Uani 1 1 d . A .
H10A H 0.3174 0.0595 0.8844 0.079 Uiso 1 1 calc R . .
C11 C 0.3830(8) 0.0978(3) 0.7741(6) 0.066(3) Uani 1 1 d . . .
H11A H 0.4486 0.1075 0.8174 0.080 Uiso 1 1 calc R A .
C12 C 0.3608(8) 0.1121(3) 0.6691(6) 0.059(2) Uani 1 1 d . A .
H12A H 0.4123 0.1319 0.6418 0.071 Uiso 1 1 calc R . .
C21 C 0.2172(10) 0.0829(3) 0.1693(9) 0.038(7) Uiso 0.60(2) 1 d PG A 1
C22 C 0.1093(8) 0.0718(3) 0.1180(11) 0.051(4) Uiso 0.60(2) 1 d PG A 1
H22A H 0.0393 0.0877 0.1247 0.061 Uiso 0.60(2) 1 calc PR A 1
C23 C 0.1038(8) 0.0373(4) 0.0570(12) 0.062(5) Uiso 0.60(2) 1 d PG A 1
H23A H 0.0300 0.0297 0.0219 0.075 Uiso 0.60(2) 1 calc PR A 1
C24 C 0.2062(10) 0.0140(3) 0.0472(9) 0.059(5) Uiso 0.60(2) 1 d PG A 1
H24A H 0.2025 -0.0095 0.0055 0.071 Uiso 0.60(2) 1 calc PR A 1
C25 C 0.3142(10) 0.0252(3) 0.0986(8) 0.046(5) Uiso 0.60(2) 1 d PG A 1
H25A H 0.3842 0.0092 0.0919 0.055 Uiso 0.60(2) 1 calc PR A 1
C26 C 0.3197(9) 0.0596(4) 0.1596(9) 0.031(4) Uiso 0.60(2) 1 d PG A 1
H26A H 0.3935 0.0672 0.1947 0.037 Uiso 0.60(2) 1 calc PR A 1
C21A C 0.2274(17) 0.0817(5) 0.1846(16) 0.037(9) Uiso 0.40(2) 1 d PG A 2
C22A C 0.1212(14) 0.0605(6) 0.1658(19) 0.072(8) Uiso 0.40(2) 1 d PG A 2
H22B H 0.0463 0.0712 0.1871 0.086 Uiso 0.40(2) 1 calc PR A 2
C23A C 0.1248(16) 0.0238(6) 0.116(2) 0.085(10) Uiso 0.40(2) 1 d PG A 2
H23B H 0.0523 0.0094 0.1029 0.102 Uiso 0.40(2) 1 calc PR A 2
C24A C 0.235(2) 0.0083(5) 0.0846(17) 0.081(9) Uiso 0.40(2) 1 d PG A 2
H24B H 0.2370 -0.0168 0.0504 0.097 Uiso 0.40(2) 1 calc PR A 2
C25A C 0.3407(14) 0.0294(7) 0.1034(18) 0.093(13) Uiso 0.40(2) 1 d PG A 2
H25B H 0.4156 0.0187 0.0820 0.111 Uiso 0.40(2) 1 calc PR A 2
C26A C 0.3371(14) 0.0661(7) 0.1534(19) 0.087(13) Uiso 0.40(2) 1 d PG A 2
H26B H 0.4096 0.0805 0.1662 0.104 Uiso 0.40(2) 1 calc PR A 2
C31 C 0.1035(6) 0.1568(2) 0.2044(5) 0.0354(18) Uani 1 1 d . A 2
C32 C -0.0127(7) 0.1437(3) 0.2219(6) 0.055(2) Uani 1 1 d . A 2
H32A H -0.0244 0.1205 0.2635 0.066 Uiso 1 1 calc R A 2
C33 C -0.1135(7) 0.1641(3) 0.1790(6) 0.060(2) Uani 1 1 d . A 2
H33A H -0.1929 0.1556 0.1945 0.072 Uiso 1 1 calc R A 2
C34 C -0.0967(7) 0.1959(2) 0.1157(6) 0.049(2) Uani 1 1 d . A 2
H34A H -0.1637 0.2081 0.0797 0.059 Uiso 1 1 calc R A 2
C35 C 0.0174(7) 0.2104(3) 0.1036(6) 0.050(2) Uani 1 1 d . A 2
H35A H 0.0285 0.2342 0.0643 0.060 Uiso 1 1 calc R A 2
C36 C 0.1152(6) 0.1912(2) 0.1472(5) 0.0383(18) Uani 1 1 d . A 2
H36A H 0.1935 0.2020 0.1378 0.046 Uiso 1 1 calc R A 2
C41 C 0.3600(6) 0.1519(2) 0.1968(5) 0.0376(19) Uani 1 1 d . A 2
C42 C 0.3630(6) 0.1542(3) 0.0840(5) 0.047(2) Uani 1 1 d . A 2
H42A H 0.3012 0.1421 0.0410 0.056 Uiso 1 1 calc R A 2
C43 C 0.4569(6) 0.1745(2) 0.0346(6) 0.050(2) Uani 1 1 d . A 2
H43A H 0.4568 0.1768 -0.0417 0.060 Uiso 1 1 calc R A 2
C44 C 0.5493(6) 0.1912(2) 0.0958(6) 0.045(2) Uani 1 1 d . A 2
H44A H 0.6131 0.2048 0.0624 0.054 Uiso 1 1 calc R A 2
C45 C 0.5475(7) 0.1877(2) 0.2063(6) 0.051(2) Uani 1 1 d . A 2
H45A H 0.6117 0.1986 0.2490 0.062 Uiso 1 1 calc R A 2
C46 C 0.4532(6) 0.1686(2) 0.2564(6) 0.044(2) Uani 1 1 d . A 2
H46A H 0.4534 0.1670 0.3328 0.053 Uiso 1 1 calc R A 2
C51 C -0.0348(6) 0.1710(2) 0.4962(5) 0.042(2) Uani 1 1 d . A 2
C52 C -0.0949(7) 0.2037(2) 0.5378(5) 0.046(2) Uani 1 1 d . A 2
H52A H -0.0501 0.2256 0.5652 0.055 Uiso 1 1 calc R A 2
C53 C -0.2208(7) 0.2040(3) 0.5392(6) 0.050(2) Uani 1 1 d . A 2
H53A H -0.2614 0.2264 0.5666 0.060 Uiso 1 1 calc R A 2
C54 C -0.2874(7) 0.1720(3) 0.5010(7) 0.059(2) Uani 1 1 d . A 2
H54A H -0.3731 0.1725 0.5010 0.071 Uiso 1 1 calc R A 2
C55 C -0.2273(8) 0.1400(3) 0.4635(7) 0.075(3) Uani 1 1 d . A 2
H55A H -0.2722 0.1177 0.4387 0.090 Uiso 1 1 calc R A 2
C56 C -0.1020(7) 0.1390(3) 0.4607(7) 0.056(2) Uani 1 1 d . A 2
H56A H -0.0625 0.1163 0.4342 0.067 Uiso 1 1 calc R A 2
C61 C 0.1655(8) 0.2160(2) 0.4198(5) 0.046(2) Uani 1 1 d . A 2
C62 C 0.0773(9) 0.2390(2) 0.3706(5) 0.054(2) Uani 1 1 d . A 2
H62A H -0.0052 0.2316 0.3741 0.065 Uiso 1 1 calc R A 2
C63 C 0.1089(10) 0.2730(3) 0.3164(6) 0.063(3) Uani 1 1 d . A 2
H63A H 0.0472 0.2887 0.2834 0.076 Uiso 1 1 calc R A 2
C64 C 0.2275(12) 0.2845(3) 0.3089(7) 0.077(3) Uani 1 1 d . A 2
H64A H 0.2470 0.3082 0.2720 0.092 Uiso 1 1 calc R A 2
C65 C 0.3180(10) 0.2615(3) 0.3556(6) 0.065(3) Uani 1 1 d . A 2
H65A H 0.4003 0.2692 0.3517 0.078 Uiso 1 1 calc R A 2
C66 C 0.2853(8) 0.2260(2) 0.4098(6) 0.052(2) Uani 1 1 d . A 2
H66A H 0.3465 0.2091 0.4392 0.063 Uiso 1 1 calc R A 2
C71 C 0.1622(6) 0.1832(2) 0.6359(5) 0.0367(18) Uani 1 1 d . A 2
C72 C 0.2426(7) 0.2119(2) 0.6682(5) 0.047(2) Uani 1 1 d . A 2
H72A H 0.2868 0.2255 0.6153 0.056 Uiso 1 1 calc R A 2
C73 C 0.2613(7) 0.2216(3) 0.7755(6) 0.051(2) Uani 1 1 d . A 2
H73A H 0.3162 0.2420 0.7959 0.061 Uiso 1 1 calc R A 2
C74 C 0.1992(8) 0.2013(3) 0.8524(6) 0.058(2) Uani 1 1 d . A 2
H74A H 0.2108 0.2080 0.9264 0.070 Uiso 1 1 calc R A 2
C75 C 0.1186(7) 0.1707(3) 0.8227(6) 0.050(2) Uani 1 1 d . A 2
H75A H 0.0774 0.1563 0.8761 0.060 Uiso 1 1 calc R A 2
C76 C 0.1005(6) 0.1620(2) 0.7161(5) 0.044(2) Uani 1 1 d . A 2
H76A H 0.0458 0.1416 0.6953 0.052 Uiso 1 1 calc R A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0311(4) 0.0299(4) 0.0382(4) 0.0012(3) 0.0036(2) -0.0012(3)
Cl1 0.0351(11) 0.0363(13) 0.0919(15) 0.0053(12) -0.0002(10) -0.0055(10)
P1 0.0273(10) 0.0343(13) 0.0366(10) -0.0035(9) -0.0002(8) 0.0011(9)
P2 0.0392(11) 0.0288(12) 0.0373(10) -0.0019(9) 0.0054(8) 0.0007(9)
N1 0.026(3) 0.041(4) 0.037(3) -0.003(3) 0.008(2) -0.001(3)
N2 0.021(3) 0.025(4) 0.053(4) 0.004(3) 0.010(3) -0.005(3)
N3 0.031(4) 0.053(5) 0.044(3) -0.008(3) 0.001(3) -0.010(3)
C1 0.026(4) 0.066(7) 0.048(4) 0.010(4) -0.005(3) -0.005(4)
C2 0.034(5) 0.063(7) 0.075(6) 0.015(5) 0.009(4) 0.011(5)
C3 0.060(6) 0.057(7) 0.059(5) 0.008(5) 0.008(4) 0.034(5)
C4 0.053(5) 0.039(6) 0.061(5) 0.005(4) 0.005(4) 0.006(5)
C5 0.037(4) 0.028(5) 0.042(4) 0.000(4) 0.002(3) 0.000(4)
C6 0.052(5) 0.025(5) 0.066(5) -0.002(4) 0.009(4) 0.004(4)
C7 0.042(5) 0.045(6) 0.056(5) 0.018(4) 0.015(4) 0.001(4)
C8 0.052(5) 0.028(5) 0.039(4) 0.001(4) 0.011(4) 0.007(4)
C9 0.074(6) 0.049(6) 0.045(5) 0.010(4) 0.007(4) 0.000(5)
C10 0.099(8) 0.056(7) 0.042(5) 0.006(5) 0.005(5) 0.015(6)
C11 0.060(6) 0.097(9) 0.041(5) 0.010(5) -0.013(4) 0.006(6)
C12 0.082(7) 0.052(6) 0.045(5) 0.011(4) 0.004(4) -0.004(5)
C31 0.036(4) 0.031(5) 0.039(4) 0.002(4) 0.004(3) -0.001(4)
C32 0.043(5) 0.053(6) 0.068(5) 0.022(5) -0.002(4) 0.005(5)
C33 0.039(5) 0.053(7) 0.086(6) 0.017(5) -0.006(4) -0.011(5)
C34 0.044(5) 0.044(6) 0.060(5) 0.016(4) -0.011(4) 0.001(4)
C35 0.050(5) 0.044(6) 0.057(5) -0.009(4) 0.007(4) 0.013(5)
C36 0.035(4) 0.026(5) 0.053(4) -0.004(4) 0.004(4) -0.005(4)
C41 0.031(4) 0.035(5) 0.048(4) 0.008(4) 0.008(3) -0.004(4)
C42 0.034(4) 0.062(6) 0.045(5) 0.004(4) 0.005(3) -0.003(4)
C43 0.040(5) 0.053(6) 0.057(5) 0.016(4) 0.010(4) 0.005(4)
C44 0.026(4) 0.043(6) 0.067(5) 0.008(4) 0.010(4) -0.005(4)
C45 0.050(5) 0.051(6) 0.052(5) 0.013(4) -0.003(4) -0.015(5)
C46 0.038(5) 0.042(5) 0.052(5) 0.003(4) 0.001(4) -0.006(4)
C51 0.038(4) 0.045(6) 0.043(4) -0.005(4) 0.007(3) 0.005(4)
C52 0.066(6) 0.034(5) 0.038(4) 0.001(4) 0.004(4) 0.001(4)
C53 0.052(5) 0.037(6) 0.062(5) -0.006(4) 0.012(4) 0.016(4)
C54 0.039(5) 0.053(7) 0.086(6) -0.015(5) -0.005(4) 0.011(5)
C55 0.053(6) 0.051(7) 0.121(8) -0.022(6) -0.011(5) -0.001(5)
C56 0.038(5) 0.037(6) 0.091(6) -0.010(5) -0.012(4) 0.006(4)
C61 0.076(6) 0.028(5) 0.033(4) -0.002(4) 0.011(4) -0.009(5)
C62 0.097(7) 0.028(5) 0.037(4) 0.005(4) 0.015(4) 0.014(5)
C63 0.103(8) 0.032(6) 0.054(5) 0.006(4) 0.021(5) 0.018(6)
C64 0.151(11) 0.033(6) 0.049(5) -0.004(5) 0.019(6) -0.021(7)
C65 0.096(8) 0.051(7) 0.049(5) -0.013(5) 0.009(5) -0.028(6)
C66 0.079(6) 0.026(5) 0.052(5) -0.003(4) 0.005(4) -0.016(5)
C71 0.038(4) 0.026(5) 0.046(4) -0.007(4) -0.010(3) 0.002(4)
C72 0.052(5) 0.050(6) 0.037(4) -0.001(4) -0.001(4) -0.006(4)
C73 0.060(5) 0.043(6) 0.049(5) -0.001(4) -0.008(4) -0.020(5)
C74 0.072(6) 0.067(7) 0.035(4) -0.002(5) -0.009(4) 0.026(6)
C75 0.044(5) 0.067(7) 0.039(5) 0.013(4) 0.002(4) -0.003(5)
C76 0.051(5) 0.038(5) 0.042(4) 0.000(4) 0.007(4) -0.012(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 H1RU 1.74(7) . ?
Ru1 N3 2.111(6) . ?
Ru1 N1 2.128(6) . ?
Ru1 N2 2.234(5) . ?
Ru1 P2 2.284(2) . ?
Ru1 P1 2.2931(18) . ?
P1 C21A 1.821(15) . ?
P1 C31 1.849(7) . ?
P1 C41 1.853(6) . ?
P1 C21 1.898(8) . ?
P2 C51 1.851(7) . ?
P2 C61 1.860(8) . ?
P2 C71 1.874(7) . ?
N1 C5 1.337(9) . ?
N1 C1 1.345(8) . ?
N2 C7 1.487(8) . ?
N2 C6 1.492(8) . ?
N3 C12 1.341(9) . ?
N3 C8 1.348(9) . ?
C1 C2 1.415(11) . ?
C2 C3 1.353(12) . ?
C3 C4 1.371(10) . ?
C4 C5 1.376(10) . ?
C5 C6 1.511(9) . ?
C7 C8 1.478(10) . ?
C8 C9 1.386(10) . ?
C9 C10 1.367(11) . ?
C10 C11 1.386(12) . ?
C11 C12 1.404(10) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C21A C22A 1.3900 . ?
C21A C26A 1.3900 . ?
C22A C23A 1.3900 . ?
C23A C24A 1.3900 . ?
C24A C25A 1.3900 . ?
C25A C26A 1.3900 . ?
C31 C36 1.374(9) . ?
C31 C32 1.385(9) . ?
C32 C33 1.404(10) . ?
C33 C34 1.349(10) . ?
C34 C35 1.369(10) . ?
C35 C36 1.362(9) . ?
C41 C46 1.373(9) . ?
C41 C42 1.403(9) . ?
C42 C43 1.402(9) . ?
C43 C44 1.377(10) . ?
C44 C45 1.375(9) . ?
C45 C46 1.391(9) . ?
C51 C56 1.378(10) . ?
C51 C52 1.398(10) . ?
C52 C53 1.396(9) . ?
C53 C54 1.385(11) . ?
C54 C55 1.362(11) . ?
C55 C56 1.390(10) . ?
C61 C62 1.379(10) . ?
C61 C66 1.379(10) . ?
C62 C63 1.381(11) . ?
C63 C64 1.376(12) . ?
C64 C65 1.383(12) . ?
C65 C66 1.432(11) . ?
C71 C72 1.371(9) . ?
C71 C76 1.417(9) . ?
C72 C73 1.380(9) . ?
C73 C74 1.376(10) . ?
C74 C75 1.409(11) . ?
C75 C76 1.364(9) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1RU Ru1 N3 89(2) . . ?
H1RU Ru1 N1 97(2) . . ?
N3 Ru1 N1 83.7(2) . . ?
H1RU Ru1 N2 166(2) . . ?
N3 Ru1 N2 77.0(2) . . ?
N1 Ru1 N2 77.4(2) . . ?
H1RU Ru1 P2 77(2) . . ?
N3 Ru1 P2 91.44(18) . . ?
N1 Ru1 P2 172.06(16) . . ?
N2 Ru1 P2 107.71(14) . . ?
H1RU Ru1 P1 90(2) . . ?
N3 Ru1 P1 172.62(17) . . ?
N1 Ru1 P1 88.96(15) . . ?
N2 Ru1 P1 102.52(15) . . ?
P2 Ru1 P1 95.70(7) . . ?
C21A P1 C31 104.5(7) . . ?
C21A P1 C41 99.1(7) . . ?
C31 P1 C41 100.7(3) . . ?
C21A P1 C21 6.4(8) . . ?
C31 P1 C21 98.5(4) . . ?
C41 P1 C21 98.2(4) . . ?
C21A P1 Ru1 111.1(6) . . ?
C31 P1 Ru1 119.4(2) . . ?
C41 P1 Ru1 119.3(2) . . ?
C21 P1 Ru1 116.6(4) . . ?
C51 P2 C61 101.5(4) . . ?
C51 P2 C71 96.4(3) . . ?
C61 P2 C71 102.0(3) . . ?
C51 P2 Ru1 125.1(3) . . ?
C61 P2 Ru1 116.2(3) . . ?
C71 P2 Ru1 111.8(2) . . ?
C5 N1 C1 117.9(7) . . ?
C5 N1 Ru1 119.1(5) . . ?
C1 N1 Ru1 122.9(6) . . ?
C7 N2 C6 113.3(6) . . ?
C7 N2 Ru1 107.4(4) . . ?
C6 N2 Ru1 110.3(4) . . ?
C12 N3 C8 118.3(7) . . ?
C12 N3 Ru1 123.6(5) . . ?
C8 N3 Ru1 117.8(5) . . ?
N1 C1 C2 121.9(8) . . ?
C3 C2 C1 118.0(8) . . ?
C2 C3 C4 120.7(8) . . ?
C3 C4 C5 118.4(8) . . ?
N1 C5 C4 123.1(7) . . ?
N1 C5 C6 116.5(6) . . ?
C4 C5 C6 120.4(7) . . ?
N2 C6 C5 113.8(6) . . ?
C8 C7 N2 111.7(5) . . ?
N3 C8 C9 122.8(7) . . ?
N3 C8 C7 115.6(6) . . ?
C9 C8 C7 121.5(7) . . ?
C10 C9 C8 118.6(8) . . ?
C9 C10 C11 120.1(8) . . ?
C10 C11 C12 118.1(8) . . ?
N3 C12 C11 122.1(8) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 P1 123.0(6) . . ?
C26 C21 P1 116.9(6) . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C24 120.0 . . ?
C23 C24 C25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C21 120.0 . . ?
C22A C21A C26A 120.0 . . ?
C22A C21A P1 122.1(11) . . ?
C26A C21A P1 117.6(11) . . ?
C23A C22A C21A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C25A C26A C21A 120.0 . . ?
C36 C31 C32 117.1(7) . . ?
C36 C31 P1 124.8(5) . . ?
C32 C31 P1 118.1(6) . . ?
C31 C32 C33 121.1(8) . . ?
C34 C33 C32 119.4(8) . . ?
C33 C34 C35 119.7(8) . . ?
C36 C35 C34 120.7(8) . . ?
C35 C36 C31 121.6(7) . . ?
C46 C41 C42 118.3(6) . . ?
C46 C41 P1 121.8(5) . . ?
C42 C41 P1 119.9(5) . . ?
C43 C42 C41 120.2(7) . . ?
C44 C43 C42 120.5(7) . . ?
C45 C44 C43 118.9(7) . . ?
C44 C45 C46 121.2(7) . . ?
C41 C46 C45 120.9(7) . . ?
C56 C51 C52 118.7(7) . . ?
C56 C51 P2 119.6(6) . . ?
C52 C51 P2 121.6(6) . . ?
C53 C52 C51 119.8(8) . . ?
C54 C53 C52 120.8(7) . . ?
C55 C54 C53 118.6(8) . . ?
C54 C55 C56 121.6(9) . . ?
C51 C56 C55 120.3(8) . . ?
C62 C61 C66 119.5(8) . . ?
C62 C61 P2 123.0(7) . . ?
C66 C61 P2 117.3(7) . . ?
C61 C62 C63 120.0(9) . . ?
C64 C63 C62 121.7(9) . . ?
C63 C64 C65 119.6(9) . . ?
C64 C65 C66 118.7(9) . . ?
C61 C66 C65 120.4(9) . . ?
C72 C71 C76 118.4(6) . . ?
C72 C71 P2 123.8(6) . . ?
C76 C71 P2 117.8(6) . . ?
C71 C72 C73 121.9(7) . . ?
C74 C73 C72 119.1(8) . . ?
C73 C74 C75 120.7(7) . . ?
C76 C75 C74 119.1(7) . . ?
C75 C76 C71 120.8(7) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2B Cl1 0.93 2.33 3.180(6) 152.5 .
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 1.519
_refine_diff_density_min -0.810
_refine_diff_density_rms 0.128
_vrf_PLAT601_k10161
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of 189.00 A**3
RESPONSE:
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly diethylether and/or ethanol). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 189.0 \%A^3^ containing approximately 41
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
_vrf_PLAT201_k10161
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 6
RESPONSE: Disorder atoms are refined as isotropic.
;
# Attachment '- 2.cif'
data_k1179a
_database_code_depnum_ccdc_archive 'CCDC 821592'
#TrackingRef '- 2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H43 N3 P2 Ru'
_chemical_formula_sum 'C48 H43 N3 P2 Ru'
_chemical_formula_weight 824.86
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 21.076(4)
_cell_length_b 9.2890(19)
_cell_length_c 20.185(4)
_cell_angle_alpha 90.00
_cell_angle_beta 93.48(3)
_cell_angle_gamma 90.00
_cell_volume 3944.4(14)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 38699
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description needle
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.389
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1704
_exptl_absorpt_coefficient_mu 0.517
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.899
_exptl_absorpt_correction_T_max 0.982
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 38699
_diffrn_reflns_av_R_equivalents 0.0761
_diffrn_reflns_av_sigmaI/netI 0.0674
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.58
_diffrn_reflns_theta_max 27.47
_reflns_number_total 9006
_reflns_number_gt 6356
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.5813P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9006
_refine_ls_number_parameters 496
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0841
_refine_ls_R_factor_gt 0.0509
_refine_ls_wR_factor_ref 0.1308
_refine_ls_wR_factor_gt 0.1154
_refine_ls_goodness_of_fit_ref 1.020
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.225840(12) 0.05083(3) 0.079258(12) 0.02733(10) Uani 1 1 d . . .
H1RU H 0.2222(14) -0.124(4) 0.0822(14) 0.033 Uiso 1 1 d . . .
P1 P 0.20730(4) 0.06142(9) 0.18748(4) 0.02793(19) Uani 1 1 d . . .
P2 P 0.33302(4) 0.02011(9) 0.07990(4) 0.0278(2) Uani 1 1 d . . .
N1 N 0.22895(12) 0.2764(3) 0.05088(14) 0.0314(6) Uani 1 1 d . . .
N2 N 0.18067(13) 0.0524(3) -0.01810(14) 0.0342(7) Uani 1 1 d . . .
H2N H 0.1726(18) -0.032(4) -0.0438(18) 0.041 Uiso 1 1 d . . .
N3 N 0.09964(15) -0.1736(3) -0.00898(17) 0.0505(8) Uani 1 1 d . . .
C1 C 0.24716(18) 0.3911(4) 0.08987(19) 0.0433(9) Uani 1 1 d . . .
H1A H 0.2673 0.3724 0.1324 0.052 Uiso 1 1 calc R . .
C2 C 0.2385(2) 0.5229(5) 0.0723(2) 0.0536(11) Uani 1 1 d U . .
H2A H 0.2506 0.5967 0.1031 0.064 Uiso 1 1 calc R . .
C3 C 0.2126(2) 0.5619(4) 0.0105(2) 0.0587(12) Uani 1 1 d U . .
H3A H 0.2074 0.6599 -0.0021 0.070 Uiso 1 1 calc R . .
C4 C 0.1946(2) 0.4514(4) -0.0315(2) 0.0532(11) Uani 1 1 d . . .
H4A H 0.1754 0.4715 -0.0744 0.064 Uiso 1 1 calc R . .
C5 C 0.20460(17) 0.3084(4) -0.01096(18) 0.0404(9) Uani 1 1 d . . .
C6 C 0.19076(18) 0.1836(4) -0.05614(18) 0.0438(9) Uani 1 1 d . . .
H6A H 0.1523 0.2043 -0.0852 0.053 Uiso 1 1 calc R . .
H6B H 0.2268 0.1691 -0.0847 0.053 Uiso 1 1 calc R . .
C7 C 0.13352(16) 0.0594(4) 0.03131(17) 0.0330(8) Uani 1 1 d . . .
H7 H 0.1122(17) 0.152(4) 0.0335(16) 0.040 Uiso 1 1 d . . .
C8 C 0.09019(16) -0.0635(4) 0.03195(18) 0.0374(8) Uani 1 1 d . . .
C9 C 0.04015(17) -0.0639(4) 0.07499(19) 0.0442(9) Uani 1 1 d . . .
H9A H 0.0338 0.0160 0.1032 0.053 Uiso 1 1 calc R . .
C10 C 0.0007(2) -0.1808(5) 0.0756(2) 0.0586(12) Uani 1 1 d . . .
H10A H -0.0331 -0.1835 0.1047 0.070 Uiso 1 1 calc R . .
C11 C 0.0106(2) -0.2949(5) 0.0335(3) 0.0732(15) Uani 1 1 d . . .
H11A H -0.0163 -0.3771 0.0329 0.088 Uiso 1 1 calc R . .
C12 C 0.0597(2) -0.2866(5) -0.0071(3) 0.0698(14) Uani 1 1 d . . .
H12A H 0.0663 -0.3655 -0.0358 0.084 Uiso 1 1 calc R . .
C21 C 0.13033(15) 0.1518(4) 0.20201(17) 0.0333(8) Uani 1 1 d . . .
C22 C 0.09056(18) 0.1095(4) 0.2511(2) 0.0473(10) Uani 1 1 d . . .
H22A H 0.1039 0.0357 0.2814 0.057 Uiso 1 1 calc R . .
C23 C 0.03120(19) 0.1747(5) 0.2563(2) 0.0602(12) Uani 1 1 d . . .
H23A H 0.0039 0.1420 0.2888 0.072 Uiso 1 1 calc R . .
C24 C 0.01221(19) 0.2849(4) 0.2149(2) 0.0568(12) Uani 1 1 d . . .
H24A H -0.0278 0.3297 0.2194 0.068 Uiso 1 1 calc R . .
C25 C 0.05081(18) 0.3306(4) 0.1671(2) 0.0466(10) Uani 1 1 d . . .
H25A H 0.0377 0.4076 0.1385 0.056 Uiso 1 1 calc R . .
C26 C 0.10950(16) 0.2645(4) 0.16033(17) 0.0346(8) Uani 1 1 d . . .
H26A H 0.1358 0.2967 0.1267 0.042 Uiso 1 1 calc R . .
C31 C 0.25987(16) 0.1630(4) 0.24829(16) 0.0322(8) Uani 1 1 d . . .
C32 C 0.24781(17) 0.3061(4) 0.26299(16) 0.0366(8) Uani 1 1 d . . .
H32A H 0.2092 0.3492 0.2462 0.044 Uiso 1 1 calc R . .
C33 C 0.29127(19) 0.3878(4) 0.30191(17) 0.0416(9) Uani 1 1 d . . .
H33A H 0.2823 0.4860 0.3107 0.050 Uiso 1 1 calc R . .
C34 C 0.34692(19) 0.3273(5) 0.32763(17) 0.0463(10) Uani 1 1 d . . .
H34A H 0.3766 0.3832 0.3540 0.056 Uiso 1 1 calc R . .
C35 C 0.35929(19) 0.1845(5) 0.31484(18) 0.0476(10) Uani 1 1 d . . .
H35A H 0.3973 0.1416 0.3333 0.057 Uiso 1 1 calc R . .
C36 C 0.31685(17) 0.1029(4) 0.27526(17) 0.0391(8) Uani 1 1 d . . .
H36A H 0.3265 0.0052 0.2663 0.047 Uiso 1 1 calc R . .
C41 C 0.19297(15) -0.1090(4) 0.23262(16) 0.0317(7) Uani 1 1 d . . .
C42 C 0.20220(17) -0.1234(4) 0.30144(17) 0.0396(8) Uani 1 1 d . . .
H42A H 0.2228 -0.0487 0.3267 0.048 Uiso 1 1 calc R . .
C43 C 0.18177(18) -0.2448(4) 0.3329(2) 0.0463(10) Uani 1 1 d . . .
H43A H 0.1872 -0.2518 0.3799 0.056 Uiso 1 1 calc R . .
C44 C 0.15378(19) -0.3552(4) 0.2974(2) 0.0494(10) Uani 1 1 d . . .
H44A H 0.1401 -0.4389 0.3195 0.059 Uiso 1 1 calc R . .
C45 C 0.14535(18) -0.3450(4) 0.22875(19) 0.0427(9) Uani 1 1 d . . .
H45A H 0.1265 -0.4223 0.2038 0.051 Uiso 1 1 calc R . .
C46 C 0.16439(16) -0.2225(4) 0.19706(18) 0.0363(8) Uani 1 1 d . . .
H46A H 0.1579 -0.2154 0.1502 0.044 Uiso 1 1 calc R . .
C51 C 0.37660(15) 0.1899(3) 0.07430(16) 0.0309(7) Uani 1 1 d . . .
C52 C 0.37911(17) 0.2570(4) 0.01302(17) 0.0370(8) Uani 1 1 d . . .
H52A H 0.3646 0.2065 -0.0259 0.044 Uiso 1 1 calc R . .
C53 C 0.4022(2) 0.3958(4) 0.0072(2) 0.0510(10) Uani 1 1 d . . .
H53A H 0.4033 0.4392 -0.0353 0.061 Uiso 1 1 calc R . .
C54 C 0.4234(2) 0.4705(4) 0.0628(2) 0.0511(10) Uani 1 1 d . . .
H54A H 0.4393 0.5658 0.0591 0.061 Uiso 1 1 calc R . .
C55 C 0.42157(18) 0.4062(4) 0.1241(2) 0.0431(9) Uani 1 1 d . . .
H55A H 0.4371 0.4571 0.1625 0.052 Uiso 1 1 calc R . .
C56 C 0.39737(16) 0.2677(4) 0.13089(18) 0.0353(8) Uani 1 1 d . . .
H56A H 0.3950 0.2264 0.1737 0.042 Uiso 1 1 calc R . .
C61 C 0.36201(15) -0.0817(3) 0.00861(16) 0.0292(7) Uani 1 1 d . . .
C62 C 0.31940(18) -0.1506(4) -0.03499(18) 0.0458(10) Uani 1 1 d . . .
H62A H 0.2751 -0.1395 -0.0302 0.055 Uiso 1 1 calc R . .
C63 C 0.34013(19) -0.2367(5) -0.0862(2) 0.0526(11) Uani 1 1 d . . .
H63A H 0.3099 -0.2826 -0.1160 0.063 Uiso 1 1 calc R . .
C64 C 0.40329(18) -0.2549(4) -0.09358(17) 0.0390(9) Uani 1 1 d . . .
H64A H 0.4173 -0.3141 -0.1282 0.047 Uiso 1 1 calc R . .
C65 C 0.44623(18) -0.1882(4) -0.05135(19) 0.0461(10) Uani 1 1 d . . .
H65A H 0.4904 -0.2005 -0.0566 0.055 Uiso 1 1 calc R . .
C66 C 0.42603(17) -0.1019(4) -0.00024(19) 0.0445(9) Uani 1 1 d . . .
H66A H 0.4567 -0.0560 0.0290 0.053 Uiso 1 1 calc R . .
C71 C 0.37897(16) -0.0812(3) 0.14538(16) 0.0299(7) Uani 1 1 d . . .
C72 C 0.44332(17) -0.0596(4) 0.16329(17) 0.0366(8) Uani 1 1 d . . .
H72A H 0.4656 0.0164 0.1435 0.044 Uiso 1 1 calc R . .
C73 C 0.47482(18) -0.1478(4) 0.20958(18) 0.0425(9) Uani 1 1 d . . .
H73A H 0.5185 -0.1312 0.2216 0.051 Uiso 1 1 calc R . .
C74 C 0.44383(18) -0.2589(4) 0.23839(18) 0.0433(9) Uani 1 1 d . . .
H74A H 0.4659 -0.3195 0.2699 0.052 Uiso 1 1 calc R . .
C75 C 0.38018(19) -0.2821(4) 0.22133(18) 0.0424(9) Uani 1 1 d . . .
H75A H 0.3584 -0.3587 0.2414 0.051 Uiso 1 1 calc R . .
C76 C 0.34788(17) -0.1945(4) 0.17520(16) 0.0345(8) Uani 1 1 d . . .
H76B H 0.3042 -0.2117 0.1637 0.041 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.02457(15) 0.03128(16) 0.02603(15) -0.00053(11) 0.00068(10) 0.00180(11)
P1 0.0260(4) 0.0313(5) 0.0266(4) -0.0010(3) 0.0026(3) -0.0001(3)
P2 0.0251(4) 0.0324(5) 0.0260(4) -0.0012(3) 0.0014(3) -0.0002(3)
N1 0.0246(15) 0.0356(15) 0.0344(16) 0.0034(13) 0.0059(12) 0.0029(12)
N2 0.0295(15) 0.0441(18) 0.0283(15) -0.0044(13) -0.0033(12) 0.0019(13)
N3 0.0402(19) 0.0437(19) 0.066(2) -0.0140(17) -0.0093(16) -0.0013(15)
C1 0.037(2) 0.051(2) 0.043(2) -0.0101(19) 0.0124(17) -0.0166(18)
C2 0.051(3) 0.066(3) 0.044(2) -0.009(2) 0.0015(19) 0.035(2)
C3 0.054(3) 0.039(2) 0.083(3) 0.017(2) 0.005(2) -0.0007(19)
C4 0.048(2) 0.060(3) 0.051(2) 0.028(2) 0.000(2) 0.002(2)
C5 0.033(2) 0.052(2) 0.037(2) 0.0078(17) 0.0044(16) 0.0036(17)
C6 0.038(2) 0.062(3) 0.0321(19) 0.0084(18) 0.0074(16) 0.0042(18)
C7 0.0236(17) 0.040(2) 0.0352(19) -0.0034(15) -0.0012(14) 0.0057(15)
C8 0.0264(18) 0.042(2) 0.042(2) 0.0032(17) -0.0096(16) 0.0019(15)
C9 0.033(2) 0.053(2) 0.046(2) 0.0026(18) -0.0031(17) -0.0015(17)
C10 0.036(2) 0.068(3) 0.071(3) 0.014(2) -0.008(2) -0.008(2)
C11 0.049(3) 0.049(3) 0.120(4) 0.006(3) -0.011(3) -0.014(2)
C12 0.045(3) 0.054(3) 0.109(4) -0.025(3) -0.009(3) -0.007(2)
C21 0.0270(17) 0.0341(18) 0.0392(19) -0.0071(15) 0.0047(15) -0.0027(14)
C22 0.040(2) 0.045(2) 0.058(3) 0.0027(19) 0.0155(19) 0.0038(18)
C23 0.043(2) 0.054(3) 0.087(3) 0.003(2) 0.034(2) 0.001(2)
C24 0.033(2) 0.045(2) 0.095(4) 0.001(2) 0.017(2) 0.0082(18)
C25 0.038(2) 0.037(2) 0.065(3) -0.0071(19) 0.0021(19) 0.0039(17)
C26 0.0322(19) 0.0349(19) 0.0369(19) -0.0012(15) 0.0035(16) 0.0013(15)
C31 0.0300(18) 0.040(2) 0.0263(17) 0.0021(15) 0.0029(14) -0.0052(15)
C32 0.035(2) 0.046(2) 0.0284(18) -0.0010(16) 0.0030(15) -0.0024(16)
C33 0.048(2) 0.043(2) 0.0343(19) -0.0052(17) 0.0079(17) -0.0077(18)
C34 0.047(2) 0.064(3) 0.0281(19) -0.0083(18) 0.0056(17) -0.019(2)
C35 0.040(2) 0.068(3) 0.034(2) 0.0010(19) -0.0025(17) -0.0056(19)
C36 0.040(2) 0.046(2) 0.0324(18) -0.0059(17) 0.0042(16) -0.0030(17)
C41 0.0266(17) 0.0337(18) 0.0351(18) 0.0016(15) 0.0051(14) 0.0005(14)
C42 0.041(2) 0.046(2) 0.0318(19) 0.0031(16) 0.0035(16) -0.0014(17)
C43 0.045(2) 0.053(2) 0.041(2) 0.0128(18) -0.0003(18) -0.0028(19)
C44 0.047(2) 0.044(2) 0.057(3) 0.017(2) 0.008(2) -0.0007(18)
C45 0.045(2) 0.0322(19) 0.051(2) 0.0017(17) 0.0055(18) -0.0038(16)
C46 0.0312(19) 0.041(2) 0.0368(19) 0.0042(16) 0.0050(15) 0.0012(15)
C51 0.0252(17) 0.0344(18) 0.0333(18) 0.0003(15) 0.0028(14) -0.0007(14)
C52 0.040(2) 0.037(2) 0.0332(19) 0.0001(15) 0.0014(16) -0.0068(16)
C53 0.060(3) 0.048(2) 0.045(2) 0.010(2) 0.007(2) -0.008(2)
C54 0.055(3) 0.037(2) 0.061(3) 0.0017(19) 0.008(2) -0.0121(18)
C55 0.039(2) 0.041(2) 0.049(2) -0.0098(18) -0.0006(18) -0.0013(17)
C56 0.035(2) 0.0363(19) 0.0350(19) -0.0070(15) 0.0060(16) 0.0031(15)
C61 0.0292(18) 0.0316(18) 0.0265(16) 0.0007(14) 0.0002(14) 0.0000(13)
C62 0.032(2) 0.058(2) 0.046(2) -0.0201(19) -0.0006(17) 0.0078(18)
C63 0.041(2) 0.065(3) 0.051(2) -0.025(2) -0.0063(19) 0.005(2)
C64 0.045(2) 0.041(2) 0.0312(19) -0.0073(15) 0.0082(17) 0.0021(17)
C65 0.034(2) 0.058(2) 0.048(2) -0.013(2) 0.0153(18) -0.0003(18)
C66 0.032(2) 0.059(2) 0.043(2) -0.0189(19) 0.0067(17) -0.0082(18)
C71 0.0331(18) 0.0329(18) 0.0237(16) -0.0050(14) 0.0012(14) 0.0044(14)
C72 0.0311(19) 0.043(2) 0.0355(19) -0.0016(16) -0.0009(15) 0.0015(15)
C73 0.036(2) 0.054(2) 0.037(2) -0.0019(18) -0.0058(16) 0.0095(18)
C74 0.048(2) 0.048(2) 0.033(2) 0.0018(17) -0.0065(17) 0.0167(18)
C75 0.052(2) 0.039(2) 0.036(2) 0.0044(16) 0.0074(18) 0.0041(18)
C76 0.0317(19) 0.0373(19) 0.0346(19) -0.0018(15) 0.0038(15) 0.0032(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 H1RU 1.63(3) . ?
Ru1 C7 2.121(3) . ?
Ru1 N2 2.131(3) . ?
Ru1 N1 2.175(3) . ?
Ru1 P1 2.2445(10) . ?
Ru1 P2 2.2761(10) . ?
P1 C31 1.860(3) . ?
P1 C41 1.860(3) . ?
P1 C21 1.865(3) . ?
P2 C51 1.832(3) . ?
P2 C71 1.848(3) . ?
P2 C61 1.856(3) . ?
N1 C5 1.353(4) . ?
N1 C1 1.365(5) . ?
N2 C7 1.452(4) . ?
N2 C6 1.463(5) . ?
N3 C8 1.337(5) . ?
N3 C12 1.348(5) . ?
C1 C2 1.285(6) . ?
C2 C3 1.378(6) . ?
C3 C4 1.371(6) . ?
C4 C5 1.404(5) . ?
C5 C6 1.493(5) . ?
C7 C8 1.463(5) . ?
C8 C9 1.407(5) . ?
C9 C10 1.368(5) . ?
C10 C11 1.383(7) . ?
C11 C12 1.361(7) . ?
C21 C22 1.393(5) . ?
C21 C26 1.397(5) . ?
C22 C23 1.399(5) . ?
C23 C24 1.365(6) . ?
C24 C25 1.367(6) . ?
C25 C26 1.396(5) . ?
C31 C32 1.389(5) . ?
C31 C36 1.404(5) . ?
C32 C33 1.394(5) . ?
C33 C34 1.374(5) . ?
C34 C35 1.379(6) . ?
C35 C36 1.388(5) . ?
C41 C46 1.392(5) . ?
C41 C42 1.397(5) . ?
C42 C43 1.376(5) . ?
C43 C44 1.366(6) . ?
C44 C45 1.389(5) . ?
C45 C46 1.377(5) . ?
C51 C52 1.389(5) . ?
C51 C56 1.399(5) . ?
C52 C53 1.386(5) . ?
C53 C54 1.371(6) . ?
C54 C55 1.376(6) . ?
C55 C56 1.393(5) . ?
C61 C62 1.377(5) . ?
C61 C66 1.385(5) . ?
C62 C63 1.398(5) . ?
C63 C64 1.359(5) . ?
C64 C65 1.355(5) . ?
C65 C66 1.394(5) . ?
C71 C76 1.395(5) . ?
C71 C72 1.397(5) . ?
C72 C73 1.382(5) . ?
C73 C74 1.369(5) . ?
C74 C75 1.382(5) . ?
C75 C76 1.384(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1RU Ru1 C7 90.6(11) . . ?
H1RU Ru1 N2 91.2(10) . . ?
C7 Ru1 N2 39.92(12) . . ?
H1RU Ru1 N1 166.9(10) . . ?
C7 Ru1 N1 83.40(12) . . ?
N2 Ru1 N1 76.68(11) . . ?
H1RU Ru1 P1 89.8(10) . . ?
C7 Ru1 P1 103.49(10) . . ?
N2 Ru1 P1 143.40(8) . . ?
N1 Ru1 P1 102.94(8) . . ?
H1RU Ru1 P2 85.6(11) . . ?
C7 Ru1 P2 152.85(10) . . ?
N2 Ru1 P2 113.19(8) . . ?
N1 Ru1 P2 94.39(7) . . ?
P1 Ru1 P2 103.37(4) . . ?
C31 P1 C41 102.49(15) . . ?
C31 P1 C21 99.02(15) . . ?
C41 P1 C21 97.88(15) . . ?
C31 P1 Ru1 122.18(11) . . ?
C41 P1 Ru1 118.85(11) . . ?
C21 P1 Ru1 112.16(12) . . ?
C51 P2 C71 103.87(15) . . ?
C51 P2 C61 101.58(15) . . ?
C71 P2 C61 96.43(14) . . ?
C51 P2 Ru1 113.13(11) . . ?
C71 P2 Ru1 123.02(11) . . ?
C61 P2 Ru1 115.64(11) . . ?
C5 N1 C1 116.0(3) . . ?
C5 N1 Ru1 116.0(2) . . ?
C1 N1 Ru1 127.7(2) . . ?
C7 N2 C6 116.8(3) . . ?
C7 N2 Ru1 69.68(17) . . ?
C6 N2 Ru1 114.7(2) . . ?
C8 N3 C12 117.5(4) . . ?
C2 C1 N1 123.6(4) . . ?
C1 C2 C3 122.8(4) . . ?
C4 C3 C2 116.3(4) . . ?
C3 C4 C5 119.6(4) . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 116.3(3) . . ?
C4 C5 C6 122.3(3) . . ?
N2 C6 C5 110.8(3) . . ?
N2 C7 C8 115.1(3) . . ?
N2 C7 Ru1 70.40(17) . . ?
C8 C7 Ru1 121.5(2) . . ?
N3 C8 C9 121.7(3) . . ?
N3 C8 C7 118.4(3) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 119.1(4) . . ?
C9 C10 C11 119.3(4) . . ?
C12 C11 C10 118.4(4) . . ?
N3 C12 C11 124.1(4) . . ?
C22 C21 C26 117.3(3) . . ?
C22 C21 P1 123.5(3) . . ?
C26 C21 P1 119.1(2) . . ?
C21 C22 C23 120.7(4) . . ?
C24 C23 C22 120.6(4) . . ?
C23 C24 C25 120.0(4) . . ?
C24 C25 C26 120.1(4) . . ?
C25 C26 C21 121.3(3) . . ?
C32 C31 C36 117.4(3) . . ?
C32 C31 P1 121.1(3) . . ?
C36 C31 P1 121.0(3) . . ?
C31 C32 C33 121.2(3) . . ?
C34 C33 C32 120.4(4) . . ?
C33 C34 C35 119.3(4) . . ?
C34 C35 C36 120.7(4) . . ?
C35 C36 C31 120.8(4) . . ?
C46 C41 C42 118.0(3) . . ?
C46 C41 P1 118.0(3) . . ?
C42 C41 P1 123.5(3) . . ?
C43 C42 C41 120.6(4) . . ?
C44 C43 C42 120.6(4) . . ?
C43 C44 C45 119.9(4) . . ?
C46 C45 C44 119.8(4) . . ?
C45 C46 C41 121.0(3) . . ?
C52 C51 C56 117.9(3) . . ?
C52 C51 P2 119.2(3) . . ?
C56 C51 P2 121.8(3) . . ?
C53 C52 C51 121.7(3) . . ?
C54 C53 C52 120.0(4) . . ?
C53 C54 C55 119.3(4) . . ?
C54 C55 C56 121.3(4) . . ?
C55 C56 C51 119.7(3) . . ?
C62 C61 C66 117.2(3) . . ?
C62 C61 P2 120.0(3) . . ?
C66 C61 P2 122.6(3) . . ?
C61 C62 C63 121.2(3) . . ?
C64 C63 C62 120.3(4) . . ?
C65 C64 C63 119.7(3) . . ?
C64 C65 C66 120.4(3) . . ?
C61 C66 C65 121.2(3) . . ?
C76 C71 C72 118.1(3) . . ?
C76 C71 P2 116.9(3) . . ?
C72 C71 P2 124.8(3) . . ?
C73 C72 C71 120.6(3) . . ?
C74 C73 C72 120.8(4) . . ?
C73 C74 C75 119.5(3) . . ?
C74 C75 C76 120.4(4) . . ?
C75 C76 C71 120.6(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N N3 0.95(4) 2.18(4) 2.719(4) 115(3) .
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 2.200
_refine_diff_density_min -0.644
_refine_diff_density_rms 0.089
# Attachment '- 3.cif'
data_k10233
_database_code_depnum_ccdc_archive 'CCDC 821593'
#TrackingRef '- 3.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C48 H41 N3 P2 Ru'
_chemical_formula_sum 'C48 H41 N3 P2 Ru'
_chemical_formula_weight 822.85
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.5061(3)
_cell_length_b 11.7305(3)
_cell_length_c 16.1489(3)
_cell_angle_alpha 88.6320(13)
_cell_angle_beta 78.8040(13)
_cell_angle_gamma 83.2330(12)
_cell_volume 2123.28(9)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 15884
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.0
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.287
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 848
_exptl_absorpt_coefficient_mu 0.480
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.585
_exptl_absorpt_correction_T_max 0.988
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 15884
_diffrn_reflns_av_R_equivalents 0.082
_diffrn_reflns_av_sigmaI/netI 0.059
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.12
_reflns_number_total 7369
_reflns_number_gt 6258
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.4490P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7369
_refine_ls_number_parameters 491
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0514
_refine_ls_R_factor_gt 0.0407
_refine_ls_wR_factor_ref 0.1128
_refine_ls_wR_factor_gt 0.1067
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_restrained_S_all 1.069
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.276621(19) 0.284235(19) 0.793309(13) 0.02510(10) Uani 1 1 d . . .
H1RU H 0.342(3) 0.203(3) 0.7143(19) 0.034(8) Uiso 1 1 d . . .
P1 P 0.46916(6) 0.24494(6) 0.81478(4) 0.02476(18) Uani 1 1 d . . .
P2 P 0.11782(6) 0.28625(6) 0.72500(4) 0.02391(18) Uani 1 1 d . . .
N1 N 0.3038(2) 0.4481(2) 0.74209(16) 0.0339(6) Uani 1 1 d . . .
N2 N 0.1805(2) 0.3886(2) 0.88910(16) 0.0317(6) Uani 1 1 d . . .
N3 N 0.2184(2) 0.1626(2) 0.88614(15) 0.0314(6) Uani 1 1 d . . .
C1 C 0.3657(3) 0.4783(3) 0.6670(2) 0.0432(8) Uani 1 1 d . . .
H1A H 0.4071 0.4191 0.6297 0.052 Uiso 1 1 calc R . .
C2 C 0.3722(4) 0.5912(4) 0.6409(3) 0.0607(11) Uani 1 1 d . . .
H2A H 0.4154 0.6090 0.5868 0.073 Uiso 1 1 calc R . .
C3 C 0.3132(4) 0.6783(4) 0.6970(3) 0.0667(13) Uani 1 1 d . . .
H3A H 0.3167 0.7565 0.6812 0.080 Uiso 1 1 calc R . .
C4 C 0.2514(4) 0.6509(3) 0.7734(3) 0.0556(10) Uani 1 1 d . . .
H4A H 0.2120 0.7102 0.8113 0.067 Uiso 1 1 calc R . .
C5 C 0.2449(3) 0.5345(3) 0.7976(2) 0.0386(8) Uani 1 1 d . . .
C6 C 0.1799(3) 0.5013(3) 0.8750(2) 0.0395(8) Uani 1 1 d . . .
H6A H 0.1375 0.5562 0.9155 0.047 Uiso 1 1 calc R . .
C7 C 0.1220(3) 0.3350(3) 0.95528(19) 0.0378(8) Uani 1 1 d . . .
H7A H 0.0683 0.3763 0.9996 0.045 Uiso 1 1 calc R . .
C8 C 0.1433(3) 0.2142(3) 0.95648(18) 0.0370(8) Uani 1 1 d . . .
C9 C 0.0980(3) 0.1465(4) 1.0248(2) 0.0494(10) Uani 1 1 d . . .
H9A H 0.0452 0.1821 1.0721 0.059 Uiso 1 1 calc R . .
C10 C 0.1278(4) 0.0302(4) 1.0252(2) 0.0586(11) Uani 1 1 d . . .
H10A H 0.0965 -0.0149 1.0721 0.070 Uiso 1 1 calc R . .
C11 C 0.2041(3) -0.0198(3) 0.9563(2) 0.0491(9) Uani 1 1 d . . .
H11A H 0.2278 -0.1002 0.9552 0.059 Uiso 1 1 calc R . .
C12 C 0.2461(3) 0.0481(3) 0.8887(2) 0.0368(7) Uani 1 1 d . . .
H12A H 0.2976 0.0117 0.8411 0.044 Uiso 1 1 calc R . .
C21 C 0.5768(2) 0.3108(3) 0.73308(18) 0.0296(7) Uani 1 1 d . . .
C22 C 0.6170(3) 0.2638(3) 0.6536(2) 0.0469(9) Uani 1 1 d . . .
H22A H 0.5966 0.1907 0.6416 0.056 Uiso 1 1 calc R . .
C23 C 0.6868(4) 0.3228(4) 0.5913(2) 0.0582(11) Uani 1 1 d . . .
H23A H 0.7136 0.2894 0.5369 0.070 Uiso 1 1 calc R . .
C24 C 0.7179(3) 0.4287(4) 0.6066(2) 0.0524(10) Uani 1 1 d . . .
H24A H 0.7655 0.4687 0.5635 0.063 Uiso 1 1 calc R . .
C25 C 0.6789(4) 0.4752(4) 0.6852(2) 0.0557(10) Uani 1 1 d . . .
H25A H 0.7005 0.5479 0.6972 0.067 Uiso 1 1 calc R . .
C26 C 0.6079(3) 0.4172(3) 0.7477(2) 0.0433(8) Uani 1 1 d . . .
H26A H 0.5802 0.4517 0.8017 0.052 Uiso 1 1 calc R . .
C31 C 0.5244(2) 0.0899(3) 0.81171(18) 0.0289(7) Uani 1 1 d . . .
C32 C 0.5184(3) 0.0246(3) 0.7425(2) 0.0368(7) Uani 1 1 d . . .
H32A H 0.4878 0.0601 0.6965 0.044 Uiso 1 1 calc R . .
C33 C 0.5569(3) -0.0927(3) 0.7399(2) 0.0473(9) Uani 1 1 d . . .
H33A H 0.5548 -0.1359 0.6912 0.057 Uiso 1 1 calc R . .
C34 C 0.5980(3) -0.1470(3) 0.8073(2) 0.0476(9) Uani 1 1 d . . .
H34A H 0.6236 -0.2270 0.8056 0.057 Uiso 1 1 calc R . .
C35 C 0.6014(3) -0.0829(3) 0.8768(2) 0.0447(8) Uani 1 1 d . . .
H35A H 0.6296 -0.1195 0.9234 0.054 Uiso 1 1 calc R . .
C36 C 0.5643(3) 0.0342(3) 0.8803(2) 0.0343(7) Uani 1 1 d . . .
H36A H 0.5661 0.0765 0.9293 0.041 Uiso 1 1 calc R . .
C41 C 0.5146(3) 0.2907(2) 0.91077(17) 0.0267(6) Uani 1 1 d . . .
C42 C 0.4268(3) 0.3373(2) 0.97675(18) 0.0288(6) Uani 1 1 d . . .
H42A H 0.3454 0.3447 0.9716 0.035 Uiso 1 1 calc R . .
C43 C 0.4579(3) 0.3734(3) 1.05051(19) 0.0332(7) Uani 1 1 d . . .
H43A H 0.3973 0.4050 1.0953 0.040 Uiso 1 1 calc R . .
C44 C 0.5746(3) 0.3639(3) 1.05899(19) 0.0350(7) Uani 1 1 d . . .
H44A H 0.5952 0.3886 1.1093 0.042 Uiso 1 1 calc R . .
C45 C 0.6631(3) 0.3175(3) 0.99322(19) 0.0341(7) Uani 1 1 d . . .
H45A H 0.7443 0.3106 0.9988 0.041 Uiso 1 1 calc R . .
C46 C 0.6339(3) 0.2815(3) 0.91995(19) 0.0325(7) Uani 1 1 d . . .
H46A H 0.6952 0.2504 0.8754 0.039 Uiso 1 1 calc R . .
C51 C 0.1469(3) 0.2976(3) 0.60866(17) 0.0290(7) Uani 1 1 d . . .
C52 C 0.2605(3) 0.2705(3) 0.56214(19) 0.0393(8) Uani 1 1 d . . .
H52A H 0.3257 0.2519 0.5901 0.047 Uiso 1 1 calc R . .
C53 C 0.2795(3) 0.2703(3) 0.4740(2) 0.0507(10) Uani 1 1 d . . .
H53A H 0.3581 0.2530 0.4423 0.061 Uiso 1 1 calc R . .
C54 C 0.1860(3) 0.2949(3) 0.4328(2) 0.0475(9) Uani 1 1 d . . .
H54A H 0.1993 0.2923 0.3729 0.057 Uiso 1 1 calc R . .
C55 C 0.0721(3) 0.3236(3) 0.4789(2) 0.0462(9) Uani 1 1 d . . .
H55A H 0.0071 0.3422 0.4506 0.055 Uiso 1 1 calc R . .
C56 C 0.0529(3) 0.3251(3) 0.56628(19) 0.0394(8) Uani 1 1 d . . .
H56A H -0.0254 0.3452 0.5977 0.047 Uiso 1 1 calc R . .
C61 C 0.0069(2) 0.4096(2) 0.75681(17) 0.0254(6) Uani 1 1 d . . .
C62 C -0.0768(2) 0.4076(3) 0.83215(18) 0.0293(7) Uani 1 1 d . . .
H62A H -0.0871 0.3370 0.8611 0.035 Uiso 1 1 calc R . .
C63 C -0.1450(3) 0.5076(3) 0.8651(2) 0.0359(7) Uani 1 1 d . . .
H63A H -0.2017 0.5049 0.9162 0.043 Uiso 1 1 calc R . .
C64 C -0.1308(3) 0.6112(3) 0.8238(2) 0.0392(8) Uani 1 1 d . . .
H64A H -0.1773 0.6796 0.8468 0.047 Uiso 1 1 calc R . .
C65 C -0.0491(3) 0.6150(3) 0.7492(2) 0.0367(7) Uani 1 1 d . . .
H65A H -0.0398 0.6860 0.7206 0.044 Uiso 1 1 calc R . .
C66 C 0.0198(3) 0.5154(3) 0.71570(19) 0.0307(7) Uani 1 1 d . . .
H66A H 0.0761 0.5190 0.6645 0.037 Uiso 1 1 calc R . .
C71 C 0.0322(3) 0.1620(2) 0.73600(17) 0.0269(6) Uani 1 1 d . . .
C72 C -0.0900(3) 0.1692(3) 0.73642(18) 0.0311(7) Uani 1 1 d . . .
H72A H -0.1351 0.2421 0.7344 0.037 Uiso 1 1 calc R . .
C73 C -0.1455(3) 0.0700(3) 0.7398(2) 0.0378(8) Uani 1 1 d . . .
H73A H -0.2287 0.0754 0.7403 0.045 Uiso 1 1 calc R . .
C74 C -0.0812(3) -0.0359(3) 0.7425(2) 0.0435(8) Uani 1 1 d . . .
H74A H -0.1201 -0.1033 0.7452 0.052 Uiso 1 1 calc R . .
C75 C 0.0395(3) -0.0446(3) 0.7412(2) 0.0417(8) Uani 1 1 d . . .
H75A H 0.0838 -0.1180 0.7425 0.050 Uiso 1 1 calc R . .
C76 C 0.0963(3) 0.0540(3) 0.73805(19) 0.0333(7) Uani 1 1 d . . .
H76A H 0.1796 0.0476 0.7373 0.040 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.02236(15) 0.02749(16) 0.02776(15) 0.00302(10) -0.01081(10) -0.00301(10)
P1 0.0220(4) 0.0267(4) 0.0277(4) 0.0023(3) -0.0103(3) -0.0030(3)
P2 0.0218(4) 0.0273(4) 0.0243(4) 0.0017(3) -0.0092(3) -0.0023(3)
N1 0.0278(13) 0.0352(15) 0.0441(15) 0.0114(12) -0.0201(12) -0.0065(11)
N2 0.0227(13) 0.0404(16) 0.0375(14) -0.0046(12) -0.0190(11) -0.0032(11)
N3 0.0283(13) 0.0379(15) 0.0309(14) 0.0043(11) -0.0123(11) -0.0059(11)
C1 0.0401(19) 0.045(2) 0.051(2) 0.0187(16) -0.0223(16) -0.0130(16)
C2 0.054(2) 0.061(3) 0.075(3) 0.037(2) -0.027(2) -0.022(2)
C3 0.073(3) 0.041(2) 0.103(4) 0.028(2) -0.051(3) -0.022(2)
C4 0.061(2) 0.029(2) 0.087(3) 0.0068(19) -0.044(2) -0.0027(18)
C5 0.0359(18) 0.0266(17) 0.062(2) -0.0009(15) -0.0321(16) -0.0011(14)
C6 0.0363(18) 0.0365(19) 0.051(2) -0.0114(15) -0.0242(16) 0.0048(15)
C7 0.0266(16) 0.059(2) 0.0303(16) -0.0064(15) -0.0114(13) -0.0040(15)
C8 0.0282(16) 0.060(2) 0.0266(16) 0.0009(15) -0.0104(13) -0.0118(15)
C9 0.0382(19) 0.083(3) 0.0321(18) 0.0080(18) -0.0108(15) -0.022(2)
C10 0.059(3) 0.082(3) 0.045(2) 0.028(2) -0.0204(19) -0.037(2)
C11 0.051(2) 0.049(2) 0.055(2) 0.0216(18) -0.0236(19) -0.0192(18)
C12 0.0319(17) 0.0385(19) 0.0444(18) 0.0136(15) -0.0174(14) -0.0076(14)
C21 0.0220(14) 0.0365(18) 0.0316(16) 0.0076(13) -0.0084(12) -0.0057(13)
C22 0.055(2) 0.047(2) 0.0386(19) 0.0018(16) -0.0029(16) -0.0135(18)
C23 0.061(2) 0.069(3) 0.038(2) 0.0038(18) 0.0065(18) -0.008(2)
C24 0.042(2) 0.067(3) 0.048(2) 0.0221(19) -0.0058(17) -0.0161(19)
C25 0.068(3) 0.054(2) 0.053(2) 0.0160(19) -0.020(2) -0.032(2)
C26 0.050(2) 0.048(2) 0.0368(18) 0.0056(15) -0.0126(15) -0.0207(17)
C31 0.0207(14) 0.0300(16) 0.0350(16) -0.0010(13) -0.0040(12) -0.0015(12)
C32 0.0395(18) 0.0368(18) 0.0354(17) 0.0001(14) -0.0100(14) -0.0047(15)
C33 0.053(2) 0.037(2) 0.050(2) -0.0091(16) -0.0066(17) -0.0004(17)
C34 0.053(2) 0.0276(18) 0.059(2) 0.0013(16) -0.0067(18) 0.0036(16)
C35 0.050(2) 0.0351(19) 0.050(2) 0.0151(16) -0.0158(17) -0.0029(16)
C36 0.0318(17) 0.0341(18) 0.0381(17) 0.0040(14) -0.0083(13) -0.0072(14)
C41 0.0281(15) 0.0248(15) 0.0301(15) 0.0040(12) -0.0117(12) -0.0061(12)
C42 0.0262(15) 0.0288(16) 0.0341(16) 0.0029(12) -0.0131(13) -0.0023(12)
C43 0.0384(18) 0.0312(17) 0.0318(16) -0.0028(13) -0.0113(13) -0.0030(14)
C44 0.0411(18) 0.0346(18) 0.0360(17) 0.0005(14) -0.0217(14) -0.0080(14)
C45 0.0271(16) 0.0389(18) 0.0416(18) 0.0064(14) -0.0176(14) -0.0087(14)
C46 0.0277(16) 0.0375(18) 0.0337(16) 0.0025(13) -0.0083(13) -0.0056(14)
C51 0.0326(16) 0.0302(16) 0.0257(15) 0.0037(12) -0.0082(12) -0.0067(13)
C52 0.0377(18) 0.047(2) 0.0315(17) 0.0051(14) -0.0071(14) -0.0004(15)
C53 0.049(2) 0.067(3) 0.0322(18) 0.0012(17) 0.0029(16) -0.0082(19)
C54 0.064(2) 0.055(2) 0.0253(16) 0.0049(15) -0.0105(17) -0.0138(19)
C55 0.053(2) 0.058(2) 0.0338(18) 0.0068(16) -0.0235(16) -0.0084(18)
C56 0.0369(18) 0.051(2) 0.0319(17) 0.0024(15) -0.0132(14) -0.0015(16)
C61 0.0227(14) 0.0274(16) 0.0305(15) 0.0000(12) -0.0153(12) -0.0044(12)
C62 0.0229(15) 0.0333(17) 0.0344(16) -0.0011(13) -0.0113(12) -0.0052(13)
C63 0.0281(16) 0.043(2) 0.0381(17) -0.0067(15) -0.0094(13) -0.0024(14)
C64 0.0322(17) 0.0361(19) 0.052(2) -0.0122(15) -0.0195(15) 0.0077(14)
C65 0.0393(18) 0.0272(17) 0.0489(19) 0.0021(14) -0.0229(15) -0.0026(14)
C66 0.0311(16) 0.0324(17) 0.0321(16) 0.0033(13) -0.0144(13) -0.0048(13)
C71 0.0279(15) 0.0286(16) 0.0254(14) -0.0004(12) -0.0086(12) -0.0030(12)
C72 0.0277(16) 0.0308(17) 0.0349(16) -0.0006(13) -0.0062(13) -0.0036(13)
C73 0.0293(16) 0.042(2) 0.0425(19) -0.0054(15) -0.0050(14) -0.0101(15)
C74 0.043(2) 0.0300(18) 0.059(2) -0.0012(16) -0.0100(17) -0.0102(15)
C75 0.047(2) 0.0241(17) 0.054(2) 0.0012(15) -0.0139(16) -0.0001(15)
C76 0.0325(17) 0.0317(17) 0.0368(17) -0.0009(13) -0.0115(13) 0.0005(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 H1RU 1.61(3) . ?
Ru1 N2 2.055(2) . ?
Ru1 N1 2.107(3) . ?
Ru1 N3 2.113(2) . ?
Ru1 P1 2.3002(7) . ?
Ru1 P2 2.3081(7) . ?
P1 C41 1.840(3) . ?
P1 C21 1.848(3) . ?
P1 C31 1.852(3) . ?
P2 C61 1.825(3) . ?
P2 C71 1.840(3) . ?
P2 C51 1.848(3) . ?
N1 C1 1.344(4) . ?
N1 C5 1.391(4) . ?
N2 C7 1.334(4) . ?
N2 C6 1.335(4) . ?
N3 C12 1.345(4) . ?
N3 C8 1.390(4) . ?
C1 C2 1.386(5) . ?
C2 C3 1.402(6) . ?
C3 C4 1.352(6) . ?
C4 C5 1.418(5) . ?
C5 C6 1.398(5) . ?
C7 C8 1.410(5) . ?
C8 C9 1.397(5) . ?
C9 C10 1.367(6) . ?
C10 C11 1.372(6) . ?
C11 C12 1.380(5) . ?
C21 C26 1.377(5) . ?
C21 C22 1.382(5) . ?
C22 C23 1.386(5) . ?
C23 C24 1.373(6) . ?
C24 C25 1.365(5) . ?
C25 C26 1.388(5) . ?
C31 C32 1.388(4) . ?
C31 C36 1.399(4) . ?
C32 C33 1.394(5) . ?
C33 C34 1.382(5) . ?
C34 C35 1.374(5) . ?
C35 C36 1.389(5) . ?
C41 C42 1.391(4) . ?
C41 C46 1.401(4) . ?
C42 C43 1.397(4) . ?
C43 C44 1.368(4) . ?
C44 C45 1.392(4) . ?
C45 C46 1.379(4) . ?
C51 C52 1.380(4) . ?
C51 C56 1.392(4) . ?
C52 C53 1.397(5) . ?
C53 C54 1.372(5) . ?
C54 C55 1.383(5) . ?
C55 C56 1.386(4) . ?
C61 C62 1.399(4) . ?
C61 C66 1.403(4) . ?
C62 C63 1.387(4) . ?
C63 C64 1.384(5) . ?
C64 C65 1.380(5) . ?
C65 C66 1.389(4) . ?
C71 C76 1.393(4) . ?
C71 C72 1.397(4) . ?
C72 C73 1.386(4) . ?
C73 C74 1.373(5) . ?
C74 C75 1.376(5) . ?
C75 C76 1.389(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1RU Ru1 N2 174.9(11) . . ?
H1RU Ru1 N1 100.8(11) . . ?
N2 Ru1 N1 78.79(10) . . ?
H1RU Ru1 N3 102.2(11) . . ?
N2 Ru1 N3 78.45(10) . . ?
N1 Ru1 N3 157.05(11) . . ?
H1RU Ru1 P1 76.4(11) . . ?
N2 Ru1 P1 108.68(7) . . ?
N1 Ru1 P1 93.61(7) . . ?
N3 Ru1 P1 90.84(7) . . ?
H1RU Ru1 P2 81.6(11) . . ?
N2 Ru1 P2 93.23(7) . . ?
N1 Ru1 P2 88.24(7) . . ?
N3 Ru1 P2 95.98(7) . . ?
P1 Ru1 P2 157.96(3) . . ?
C41 P1 C21 100.29(13) . . ?
C41 P1 C31 101.42(13) . . ?
C21 P1 C31 104.87(13) . . ?
C41 P1 Ru1 122.10(9) . . ?
C21 P1 Ru1 112.13(9) . . ?
C31 P1 Ru1 113.90(10) . . ?
C61 P2 C71 104.90(13) . . ?
C61 P2 C51 102.44(13) . . ?
C71 P2 C51 98.36(13) . . ?
C61 P2 Ru1 111.39(9) . . ?
C71 P2 Ru1 119.14(9) . . ?
C51 P2 Ru1 118.37(10) . . ?
C1 N1 C5 118.5(3) . . ?
C1 N1 Ru1 130.3(2) . . ?
C5 N1 Ru1 111.3(2) . . ?
C7 N2 C6 128.5(3) . . ?
C7 N2 Ru1 115.7(2) . . ?
C6 N2 Ru1 115.7(2) . . ?
C12 N3 C8 117.2(3) . . ?
C12 N3 Ru1 130.8(2) . . ?
C8 N3 Ru1 112.0(2) . . ?
N1 C1 C2 123.5(4) . . ?
C1 C2 C3 118.0(4) . . ?
C4 C3 C2 120.0(4) . . ?
C3 C4 C5 120.6(4) . . ?
N1 C5 C6 117.6(3) . . ?
N1 C5 C4 119.4(3) . . ?
C6 C5 C4 123.0(3) . . ?
N2 C6 C5 116.7(3) . . ?
N2 C7 C8 117.0(3) . . ?
N3 C8 C9 119.7(3) . . ?
N3 C8 C7 116.5(3) . . ?
C9 C8 C7 123.8(3) . . ?
C10 C9 C8 121.6(4) . . ?
C9 C10 C11 118.4(3) . . ?
C10 C11 C12 119.3(4) . . ?
N3 C12 C11 123.9(3) . . ?
C26 C21 C22 117.9(3) . . ?
C26 C21 P1 119.2(2) . . ?
C22 C21 P1 122.4(2) . . ?
C21 C22 C23 120.4(4) . . ?
C24 C23 C22 121.3(4) . . ?
C25 C24 C23 118.5(3) . . ?
C24 C25 C26 120.6(4) . . ?
C21 C26 C25 121.3(3) . . ?
C32 C31 C36 118.3(3) . . ?
C32 C31 P1 119.8(2) . . ?
C36 C31 P1 121.8(2) . . ?
C31 C32 C33 120.6(3) . . ?
C34 C33 C32 120.7(3) . . ?
C35 C34 C33 118.8(3) . . ?
C34 C35 C36 121.4(3) . . ?
C35 C36 C31 120.1(3) . . ?
C42 C41 C46 118.6(3) . . ?
C42 C41 P1 118.6(2) . . ?
C46 C41 P1 122.8(2) . . ?
C41 C42 C43 120.3(3) . . ?
C44 C43 C42 120.7(3) . . ?
C43 C44 C45 119.4(3) . . ?
C46 C45 C44 120.6(3) . . ?
C45 C46 C41 120.4(3) . . ?
C52 C51 C56 118.9(3) . . ?
C52 C51 P2 120.7(2) . . ?
C56 C51 P2 120.3(2) . . ?
C51 C52 C53 120.1(3) . . ?
C54 C53 C52 120.7(3) . . ?
C53 C54 C55 119.7(3) . . ?
C54 C55 C56 119.8(3) . . ?
C55 C56 C51 120.9(3) . . ?
C62 C61 C66 118.1(3) . . ?
C62 C61 P2 120.7(2) . . ?
C66 C61 P2 119.9(2) . . ?
C63 C62 C61 120.8(3) . . ?
C64 C63 C62 120.3(3) . . ?
C65 C64 C63 119.8(3) . . ?
C64 C65 C66 120.4(3) . . ?
C65 C66 C61 120.6(3) . . ?
C76 C71 C72 118.7(3) . . ?
C76 C71 P2 116.9(2) . . ?
C72 C71 P2 124.2(2) . . ?
C73 C72 C71 120.1(3) . . ?
C74 C73 C72 120.5(3) . . ?
C73 C74 C75 120.2(3) . . ?
C74 C75 C76 120.0(3) . . ?
C75 C76 C71 120.5(3) . . ?
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full 25.12
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max 0.765
_refine_diff_density_min -0.881
_refine_diff_density_rms 0.077
_vrf_PLAT601_k10233
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of 245.00 A**3
RESPONSE: During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly diethylether/pentane). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 245 \%A^3^ containing approximately 33
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;